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建立了茶叶中三氯杀螨醇残留量的高效液相色谱快速检测方法。选择丙酮:正己烷(1:2,V/V)对不同茶叶中三氯杀螨醇农药残留进行提取,经浓硫酸净化,1 mL甲醇定容后供高效液相色谱检测。Agilent Acclaim TM 120 C_(18)色谱柱(250×4.6,5μm)分离,流动相为乙腈-水(85:15,V/V)混合溶剂,梯度洗脱。对不同茶叶类型,提取、净化条件进行考察优化。结果表明,标准工作曲线,在0.02~5 mg/kg范围内,三氯杀螨醇线性关系良好(r为0.9999),方法定量限为0.05 mg/kg。在绿茶、红茶、黄茶、青茶、白茶、黑茶6种茶叶中4个添加水平0.05,0.1,5,50 mg/kg的平均回收率范围分别为91.8%~108.3%,88.8%~102.5%,83.7%~94.3%,80.9%~84.2%,相对标准偏差在1.2%~14%之间(n=6)。
A rapid method for the determination of dicofol residue in tea by high performance liquid chromatography was established. Acetone: n-hexane (1: 2, V / V) was used to extract the residues of dicofol in different tea leaves. After purification by concentrated sulfuric acid, 1 mL of methanol was determined for high performance liquid chromatography. The Agilent Acclaim ™ 120 C 18 column (250 × 4.6, 5 μm) was separated on a mobile phase of acetonitrile-water (85:15, V / V) mixed solvent with gradient elution. Different types of tea, extraction, purification conditions to investigate and optimize. The results showed that the standard working curve showed good linearity (r = 0.9999) for dicofol within the range of 0.02-5 mg / kg, and the limit of quantification was 0.05 mg / kg. The average recoveries of four spiked levels of green tea, black tea, yellow tea, green tea, white tea and black tea were 91.8% -108.3% and 88.8% -102.5 %, 83.7% ~ 94.3% and 80.9% ~ 84.2%, respectively. The relative standard deviations were between 1.2% and 14% (n = 6).